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J Pharm Biomed Anal


Title:Headspace solid-phase microextraction-gas chromatography-mass spectrometry characterization of propolis volatile compounds
Author(s):Pellati F; Prencipe FP; Benvenuti S;
Address:"Department of Life Sciences, University of Modena and Reggio Emilia, Via G. Campi 183, 41125 Modena, Italy. federica.pellati@unimore.it"
Journal Title:J Pharm Biomed Anal
Year:2013
Volume:20130603
Issue:
Page Number:103 - 111
DOI: 10.1016/j.jpba.2013.05.045
ISSN/ISBN:1873-264X (Electronic) 0731-7085 (Linking)
Abstract:"In this study, a novel and efficient method based on headspace solid-phase microextraction (HS-SPME), followed by gas chromatography-mass spectrometry (GC-MS), was developed for the analysis of propolis volatile compounds. The HS-SPME procedure, whose experimental parameters were properly optimized, was carried out using a 100 mum polydimethylsiloxane (PDMS) fiber. The GC-MS analyses were performed on a HP-5 MS cross-linked 5% diphenyl-95% dimethyl polysiloxane capillary column (30 m x 0.25 mm I.D., 1.00 mum film thickness), under programmed-temperature elution. Ninety-nine constituents were identified using this technique in the samples of raw propolis collected from different Italian regions. The main compounds detected include benzoic acid (0.87-30.13%) and its esters, such as benzyl benzoate (0.16-13.05%), benzyl salicylate (0.34-1.90%) and benzyl cinnamate (0.34-3.20%). Vanillin was detected in most of the samples analyzed in this study (0.07-5.44%). Another relevant class of volatile constituents is represented by sesquiterpene hydrocarbons, such as delta-cadinene (1.29-13.31%), gamma-cadinene (1.36-8.85%) and alpha-muurolene (0.78-6.59%), and oxygenated sesquiterpenes, such as beta-eudesmol (2.33-12.83%), T-cadinol (2.73-9.95%) and alpha-cadinol (4.84-9.74%). Regarding monoterpene hydrocarbons, they were found to be present at low level in the samples analyzed in this study, with the exception of one sample from Southern Italy, where alpha-pinene was the most abundant constituent (13.19%). The results obtained by HS-SPME-GC-MS were also compared with those of hydrodistillation (HD) coupled with GC-MS. The HS-SPME-GC-MS method developed in this study allowed us to determine the chemical fingerprint of propolis volatile constituents, thus providing a new and reliable tool for the complete characterization of this biologically active apiary product"
Keywords:Dimethylpolysiloxanes/chemistry Gas Chromatography-Mass Spectrometry/*methods Italy Propolis/*chemistry Solid Phase Microextraction/*methods Volatile Organic Compounds/*chemistry Dvb-car-pdms Gas chromatography Hd Hs Lri Mass spectrometry Pdms Propolis So;
Notes:"MedlinePellati, Federica Prencipe, Francesco Pio Benvenuti, Stefania eng Research Support, Non-U.S. Gov't England 2013/06/29 J Pharm Biomed Anal. 2013 Oct; 84:103-11. doi: 10.1016/j.jpba.2013.05.045. Epub 2013 Jun 3"

 
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